CN104276841B - A kind of zeolite slag-based adsorptive type granule electrode and preparation method thereof - Google Patents
A kind of zeolite slag-based adsorptive type granule electrode and preparation method thereof Download PDFInfo
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- CN104276841B CN104276841B CN201310275575.XA CN201310275575A CN104276841B CN 104276841 B CN104276841 B CN 104276841B CN 201310275575 A CN201310275575 A CN 201310275575A CN 104276841 B CN104276841 B CN 104276841B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
Zeolite slag-based adsorptive type granule electrode that the present invention relates to a kind of 3 D electrode reactor and preparation method thereof: be made up of zeolite slag, shale, pore former, activator, by weight percentage, dry thin Zeolite mineral solid impurity particle is 50-60%, dry thin shale is 10-20%, pore former is 10-20%, activator is 10-20%.Zeolite slag adsorptive type granule electrode porous of the present invention, and aperture is large, having very large specific surface area, very strong adsorptivity, electroconductibility and catalytic, is a kind of new and effective granule electrode.A kind of zeolite slag-based adsorptive type granule electrode provided by the invention and preparation method thereof, makes full use of the slag-zeolite slag produced in zeolite exploitation and screening process, both can turn waste into wealth, and can reduce again the pollution of environment, solve the problems such as land seizure.
Description
Technical field
The invention belongs to technical field of waste water processing, particularly a kind of zeolite slag-based adsorptive type granule electrode for the treatment of hardly degraded organic substance in municipal effluent and preparation method thereof.
Background technology
Zeolite can produce a large amount of zeolite slags in exploitation and screening process, and these slags have good absorption property, if reasonably do not utilized, can take a large amount of cultivated areas on the one hand, pollute the environment on the other hand, destroy ecotope around.The approach seeking to effectively utilize zeolite slag has become a focus of research.According to document, the content of general zeolite slag Si, Fe, Al is higher, and these elements are also exactly activation promotor compositions prepared by granule electrode.Therefore utilize the granule electrode of these utilized units usually synthesizing efficient, the environmental protection in zeolite slag, for the treatment of municipal effluent, red mud can be made to be utilized effectively, thus reach the object of " treatment of wastes with processes of wastes against one another ", obtain good economic benefit.
Summary of the invention
To the object of the invention is with zeolite slag, for matrix, to provide a kind of zeolite slag-based adsorptive type granule electrode and preparation method thereof.Granule electrode material provided by the present invention, can organism effectively in degrading waste water as the working electrode of 3 D electrode reactor, and current efficiency is high, and energy consumption is low.
A kind of zeolite slag-based adsorptive type granule electrode, according to weight percent meter, dry thin Zeolite mineral solid impurity particle accounts for 50-60%, dry carefully shale accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%.
Described pore former can be the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in ZnO.
Described zeolite slag is that zeolite can produce a large amount of slags in exploitation and screening process, and these slags have good absorption property.
The preparation method of above-mentioned zeolite slag-based adsorptive type granule electrode, comprises the steps:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, pore former and the activator in thin for the drying in steps A Zeolite mineral solid impurity particle, step B according to certain weight percent, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
According to weight percent meter, dry thin Zeolite mineral solid impurity particle accounts for 50-60%, dry carefully shale accounts for 10-20%, pore former accounts for 10-20%, activator accounts for 10-20%.
Described pore former can be the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
Described activator can be Fe
3o
4, Fe
2o
3,mnO
2, one in ZnO.
The zeolite slag-based adsorptive type granule electrode prepared by above-mentioned preparation method, getting solid waste zeolite slag is raw material.Containing multiple element in zeolite slag, wherein the content of Al, Zn is higher, and these elements are also exactly activation promotor compositions prepared by granule electrode.Zeolite slag basal granule sub-electrode particle surface is rough, have good absorption, removal effect, and the stacking of zeolite slag not only needs fund and large-area storage yard to the pollution substance in waste water, and contaminate environment.Utilize zeolite slag to make the particle-catalytic electrode of three-diemsnional electrode, can turn waste into wealth, reduce the problem such as pollution, appropriation of land of environment.
Zeolite slag-based adsorptive type granule electrode provided by the invention and preparation method thereof, meets the environmental protection policy of current national energy-saving and emission-reduction.The granule electrode porous of preparation, and aperture is large, having very large specific surface area, very strong absorption property, good electroconductibility and catalytic performance, is a kind of new and effective granule electrode.
Below in conjunction with embodiment, the invention will be further described.
Embodiment
Embodiment one:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, powdered carbon and the Fe in thin for the drying in steps A Zeolite mineral solid impurity particle, step B
3o
4according to the weight percent of 50%:20%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 95%.
Embodiment two:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, saw dust and the Fe in thin for the drying in steps A Zeolite mineral solid impurity particle, step B
2o
3according to the weight percent of 55%:15%:15%:15%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Embodiment three:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, starch and the MnO in thin for the drying in steps A Zeolite mineral solid impurity particle, step B
2according to the weight percent of 60%:15%:15%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Embodiment four:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, starch and the MnO in thin for the drying in steps A Zeolite mineral solid impurity particle, step B
2according to the weight percent of 60%:10%:10%:20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 96%.
Embodiment five:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, the thin shale of drying, polyvinyl alcohol (PVA) and ZnO by thin for the drying in steps A Zeolite mineral solid impurity particle, step B, according to the weight percent of 55%:15%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 96%.
Embodiment six:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, the thin shale of drying, polyvinyl butyral acetal (PVB) and ZnO by thin for the drying in steps A Zeolite mineral solid impurity particle, step B, according to the weight percent of 55%:15%:20%:10%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 97%.
Embodiment seven:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion (washing, the object of soaking are desorption of impurities), dry at 120 DEG C, then cross 60 mesh sieves, get the thin Zeolite mineral solid impurity particle of drying for subsequent use in baking oven;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale for subsequent use;
C, by the thin shale of drying, polystyrene and the ZnO in thin for the drying in steps A Zeolite mineral solid impurity particle, step B according to the weight percent of 55%:10%:15%:20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 20min, rise to 1050 DEG C of roasting 30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
Get the zeolite slag-based adsorptive type granule electrode 5.0g prepared in above-described embodiment, be filled in reactor, obtained 3 D electrode reactor, is 6.0V at voltage, and when electric current is 0.2A, energising degraded 30ml dyeing waste water 45min, CODcr clearance reaches 94%.
Claims (6)
1. a zeolite slag-based adsorptive type granule electrode, is characterized in that: according to weight percent meter, comprises dry thin Zeolite mineral solid impurity particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%.
2. zeolite slag-based adsorptive type granule electrode as claimed in claim 1, is characterized in that: pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
3. zeolite slag-based adsorptive type granule electrode as claimed in claim 1, is characterized in that: activator is Fe
3o
4, Fe
2o
3, MnO
2, one in ZnO.
4. a preparation method for zeolite slag-based adsorptive type granule electrode, is characterized in that, comprise the following steps:
A, Zeolite mineral solid impurity particle ball milling in ball mill, washing after taking out, immersion, dry at 120 DEG C in baking oven, then crosses 60 mesh sieves, gets dry thin Zeolite mineral solid impurity particle;
B, shale are put in 120 DEG C of oven dry in baking oven, are pulverized by the shale of oven dry in mortar, then cross 60 mesh sieves, get dry thin shale;
C, by the thin shale of drying, pore former and the activator in thin for the drying in steps A Zeolite mineral solid impurity particle, step B according to certain weight percent, comprise dry thin Zeolite mineral solid impurity particle 50-60%, dry thin shale 10-20%, pore former 10-20%, activator 10-20%, mix and stir, being squeezed into raw material ball;
D, by the raw material ball in step C in an oven 120 DEG C dry 24 hours;
E, by step D dry after raw material ball, be placed in High Temperature Furnaces Heating Apparatus and rise to 300 DEG C from room temperature with 120 DEG C/h, heating 2h, then 550 DEG C are risen to 60 DEG C/h, activation 10-30min, rise to 1050 DEG C of roasting 10-30min with 300 DEG C/h again, naturally cool to room temperature, obtain zeolite slag-based adsorptive type granule electrode material.
5. the preparation method of zeolite slag-based adsorptive type granule electrode as claimed in claim 4, is characterized in that: described pore former is the one in powdered carbon, saw dust, starch, polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), granules of polystyrene.
6. the preparation method of zeolite slag-based adsorptive type granule electrode as claimed in claim 4, is characterized in that: described activator is Fe
3o
4, Fe
2o
3, MnO
2, one in ZnO.
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EP0364297B1 (en) * | 1988-10-14 | 1994-01-26 | Kureha Kagaku Kogyo Kabushiki Kaisha | Porous carbon electrode substrates for fuel cells |
CN102746022A (en) * | 2011-12-29 | 2012-10-24 | 西安建筑科技大学 | Preparation method for Al2O3 ceramic material having controllable bimodal porous structure |
CN102951925A (en) * | 2012-11-28 | 2013-03-06 | 东北大学 | Diatomaceous earth matrix porous material with humidifying function and preparation method thereof |
CN103113129A (en) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | Preparation method and application of hierarchical porous bioactive ceramic |
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JP2004262730A (en) * | 2003-03-04 | 2004-09-24 | Asahi Glass Co Ltd | Method for manufacturing silicon carbide-silicon nitride combined porous body |
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Publication number | Priority date | Publication date | Assignee | Title |
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EP0364297B1 (en) * | 1988-10-14 | 1994-01-26 | Kureha Kagaku Kogyo Kabushiki Kaisha | Porous carbon electrode substrates for fuel cells |
CN102746022A (en) * | 2011-12-29 | 2012-10-24 | 西安建筑科技大学 | Preparation method for Al2O3 ceramic material having controllable bimodal porous structure |
CN102951925A (en) * | 2012-11-28 | 2013-03-06 | 东北大学 | Diatomaceous earth matrix porous material with humidifying function and preparation method thereof |
CN103113129A (en) * | 2013-01-31 | 2013-05-22 | 华南理工大学 | Preparation method and application of hierarchical porous bioactive ceramic |
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